电感耦合等离子体质谱法同时测定布南色林原料药中12种金属元素含量  

Simultaneous Determination of 12 Metal Elements in Blonanserin Active Pharmaceutical Ingredients by ICP-MS

作　　者：裴丽娟[1] 杨继章[1] 李建[1] 李卓 徐艳梅 PEI Lijuan;YANG Jizhang;LI Jian;LI Zhuo;XU Yanmei(Department of Pharmacy,The First Hospital of Hebei Medical University,Shijiazhuang,Hebei,China 050031;Hebei Institute for Drug and Medical Device Control,Shijiazhuang,Hebei,China 050200)

机构地区：[1]河北医科大学第一医院药学部,河北石家庄050031 [2]河北省药品医疗器械检验研究院,河北石家庄050200

出　　处：《中国药业》2022年第20期65-68,共4页China Pharmaceuticals

摘　　要：目的建立同时测定布南色林原料药中12种金属元素含量的电感耦合等离子体质谱(ICP-MS)法。方法以硝酸为消解体系,采用微波消解法处理样品,以^(103)Rh和^(187)Re为内标,等离子体流量为18 L/min,雾化气流速为0.94 L/min,辅助气流量为1.2 L/min,射频功率为1.6 kW,模拟电压为-1635 V,脉冲电压为800 V。结果锂(Li)、铬(Cr)、钴(Co)、镍(Ni)、铜(Cu)、银(Ag)、镉(Cd)、钡(Ba)、铅(Pb)、铈(Ce)、钬(Ho)、镥(Lu)质量浓度均在0.5~80 ng/mL范围内与仪器响应值/内标测定值线性关系良好(r≥0.9996);检测限为0.001~0.147 ng/mL;精密度、稳定性、重复性试验结果的RSD均小于3.5%;平均回收率为91.29%~94.59%,RSD为1.93%~2.79%(n=9);3批样品中均仅检出Ni和Cu,平均含量分别为22.64 ng/g和12.10 ng/g。结论该方法操作简单,分析快速,测定结果准确,适用于同时测定布南色林原料药中多种金属元素的含量。Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for the simultaneous determination of 12 metal elements in blonanserin active pharmaceutical ingredients(API).Methods With nitric acid as the digestion system,the samples were processed by microwave digestion.The internal standards were^(103)Rh and^(187)Re,the plasma flow rate was 18 L/min,the atomizing gas flow rate was 0.94 L/min,the flow rate of auxiliary gas was 1.2 L/min,the radio frequency(RF)power was 1.6 kW,the simulation voltage was-1635 V,and the pulse voltage was 800 V.Results The mass concentration of lithium(Li),chromium(Cr),cobalt(Co),nickel(Ni),copper(Cu),silver(Ag),cadmium(Cd),barium(Ba),lead(Pb),cerium(Ce),holmium(Ho)and lutetium(Lu)showed a good linear relationship with the instrument response value/internal standard determination value in the range of 0.5-80 ng/mL(r≥0.9996).The limit of detection(LOD)was in the range of 0.001-0.147 ng/mL.The RSDs of precision,stability and repeatability tests were less than 3.5%.The average recoveries of the 12 metal elements were in the range of 91.29%-94.59%with RSDs of 1.93%-2.79%(n=9).Only Ni and Cu were detected in three batches of samples,and the average contents of Ni and Cu were 22.64 ng/g and 12.10 ng/g,respectively.Conclusion The method is simple,rapid,accurate and suitable for the simultaneous determination of multiple metal elements in blonanserin API.

关 键 词：布南色林 原料药 电感耦合等离子体质谱法 金属元素 含量测定 质量控制 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]